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31.
New methods are described for the iodometric microdetermination of arsenic in organic compounds after wet digestion or oxygen flask combustion. After evaporation of the arsenic solution to dryness and dissolution of the residue in water, acetone is added and the solution is treated with iodide-iodate and the iodine liberated (by the interfering acids and the first dissociation step of arsenic acid) is reduced with thiosulphate. The KH(2)AsO(4) left is then reacted with zinc sulphate in presence of excess of KI and KIO(3). Acetone is added and the liberated iodine is titrated with thiosulphate. This titration corresponds to the second and third dissociation steps of arsenic acid and is used to calculate the arsenic content of the compound. When arsenicals not containing sulphur are decomposed by the oxygen flask method, the arsenic acid solution obtained is reacted directly with zinc sulphate in presence of KI and KIO(3) and the iodine released is titrated with thiosulphate. In this case, the titration corresponds to all three dissociation steps of arsenic acid. The average recoveries obtained by the two methods are 99.5 and 99.9%, respectively. 相似文献
32.
Mona H. N. Arsanious Leila S. Boulos 《Monatshefte für Chemie / Chemical Monthly》2006,137(9):1177-1184
Summary. The reaction of dibenzoyldiazine with phosphorus ylides afforded the new 2-[(benzoylhydrazono)phenylalkyl]but-2-enedioic acid
dialkylesters. Moreover, ethyl-2(triphenylphosphoranylidene)propionate reacts with dibenzoyldiazine to give the olefinic compound
and triphenylphosphine oxide. On the other hand, oxovinylidene-triphenylphosphorane reacts with dibenzoyldiazine to give a
new phosphorane adduct. Trialkyl phosphites react with dibenzoyldiazine to yield the dialkyl phosphonate products. The reaction
of dibenzoylhydrazide with Wittig reagents gave rise to the new 3,7-diphenylpyrazolo[1,2-α]pyrazole-1,5-diones. Possible reaction mechanisms are considered,
and the structural assignments are based on analytical and spectroscopic results. 相似文献
33.
Alexandre Dhotel Laurent Delbreilh Boulos Youssef Jinyue Jiang Gérard Coquerel Jean-Marc Saiter Li Tan 《Journal of Thermal Analysis and Calorimetry》2013,112(1):301-305
We report here a simple pathway to thermally assemble acene-based molecules into large crystals without modification of their chemical structures. Differential scanning calorimetry was used to characterize properly thermal events occurring during successive heating and cooling processes. More interestingly, observations by means of polarized light microscopy (POM) revealed that a spontaneous formation of screw dislocations within crystals during the isothermal treatment triggered a structural reorganization by forming large and well-defined spiral architectures. After this reorganization, new crystals showed an excellent ordering in both vertical and horizontal directions. Due to the richness in pi-electrons of acene-based molecules, we expect this work of importance to organic electronics, especially in the design of new molecular building blocks and investigation of their assembly into sophisticated supramolecular structures. 相似文献
34.
Leila S. Boulos Mona H. N. Arsanious Ewies F. Ewies 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):275-290
The reaction of 2-phenyl-5-(4H)-oxazolone 1 and its 4-benzylidene derivative 2 with oxovinylidenetriphenylphosphorane 3 afforded 2-phenylfuro [3,2-d] [1,3]oxazol-5-(6H)-one 6 and 2,7-diphenyl-5H-pyrano[3,2-d][1,3]oxazol-5-one 7 along with triphenylphosphine. Alternatively, when 2-phenyl-5-(4H)-oxazolone 1 reacts with phosphorus ylides 4a–f the corresponding new phosphorane, the cyclic and/or the olefinic adducts were obtained. Moreover, oxazolone reacts with N-(triphenylphosphoranylidene)aniline 5 to give the new imino product 14 together with triphenylphosphine oxide. Possible reaction mechanisms are considered and the structural assignments are based on analytical and spectroscopic results. Biological evaluations of the new products are also studied. 相似文献
35.
36.
Abe F Albrow MG Amendolia SR Amidei D Antos J Anway-Wiese C Apollinari G Areti H Auchincloss P Austern M Azfar F Azzi P Bacchetta N Badgett W Bailey MW Bao J de Barbaro P Barbaro-Galtieri A Barnes VE Barnett BA Bartalini P Bauer G Baumann T Bedeschi F Behrends S Belforte S Bellettini G Bellinger J Benjamin D Benlloch J Bensinger J Benton D Beretvas A Berge JP Bertolucci S Bhatti A Biery K Binkley M Bird F Bisello D Blair RE Blocker C Bodek A Bolognesi V Bortoletto D Boswell C Boulos T 《Physical review D: Particles and fields》1994,50(5):2966-3026
37.
Abe F Albrow M Amidei D Anway-Wiese C Apollinari G Areti H Auchincloss P Azfar F Azzi P Bacchetta N Badgett W Bailey MW Bao J de Barbaro P Barbaro-Galtieri A Barnes VE Barnett BA Bartalini P Bauer G Baumann T Bedeschi F Behrends S Belforte S Bellettini G Bellinger J Benjamin D Benlloch J Benton D Beretvas A Berge JP Bertolucci S Bhatti A Biery K Binkley M Bird F Bisello D Blair RE Blocker C Bodek A Bolognesi V Bortoletto D Boswell C Boulos T Brandenburg G Buckley-Geer E Budd HS Burkett K 《Physical review letters》1994,72(22):3456-3460
38.
Abe F Albrow M Amidei D Anway-Wiese C Apollinari G Areti H Auchincloss P Azfar F Azzi P Bacchetta N Badgett W Bailey MW Bao J de Barbaro P Barbaro-Galtieri A Barnes VE Barnett BA Bartalini P Bauer G Baumann T Bedeschi F Behrends S Belforte S Bellettini G Bellinger J Benjamin D Benlloch J Benton D Beretvas A Berge JP Bertolucci S Bhatti A Biery K Binkley M Bird F Bisello D Blair RE Blocker C Bodek A Bolognesi V Bortoletto D Boswell C Boulos T Brandenburg G Buckley-Geer E Budd HS Burkett K 《Physical review letters》1994,72(19):3004-3008
39.
Abe F Albrow M Akimoto H Amidei D Anway-Wiese C Apollinari G Areti H Auchincloss P Azfar F Azzi P Bacchetta N Badgett W Bailey MW Bao J de Barbaro P Barbaro-Galtieri A Barnes VE Barnett BA Bauer G Baumann T Bedeschi F Behrends S Belforte S Bellettini G Bellinger J Benjamin D Benlloch J Benton D Beretvas A Berge JP Bertolucci S Bhatti A Biery K Binkley M Bird F Bisello D Blair RE Blocker C Bodek A Bolognesi V Bortoletto D Boswell C Boulos T Brandenburg G Bromberg C Buckley-Geer E Budd HS 《Physical review letters》1993,71(16):2542-2546
40.
Complex impedance plots for a 25 Na2O?75 SiO2 glass exposed to the ambient atmosphere indicate the presence of a relaxation at frequencies well below those for the electrical relaxation of the bulk material, but above the frequencies where electrode polarization takes place. This low frequency relaxation is shown to occur in a high resistivity surface layer having a thickness a few times 0.1 μm and formed by the action of atmospheric water vapor. The rate of growth of the surface layer could be monitored by means of the impedance measurements and was found to decrease with the duration of exposure of the glass to the laboratory atmosphere. Complex impedance plots for a chemically durable lithium aluminosilicate glass indicate that the hydrated surface layer thickness is much smaller than in the 25 Na2O?75 SiO2 glass. 相似文献